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Recovery and utilization method for copper bearing spent acid solution from sodium saccharin production process

A technology of waste acid liquid and sodium saccharin, applied in chemical instruments and methods, multi-stage water/sewage treatment, water/sludge/sewage treatment, etc. Complete and other problems, to achieve the effect of considerable economic benefits, high product quality and simple process

Inactive Publication Date: 2004-11-03
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can separate acid and copper salt, the separation process is only based on the concentration difference, the separation is not complete, the processing capacity is small, the acid has a 20% loss, the copper ion has a 10% loss, and the equipment is expensive.
The current reverse osmosis technology and inorganic membrane technology are still unable to deal with waste liquid with such a high acid content, so it is of great significance to study this to obtain a suitable method to treat this kind of waste acid liquid
[0003] Vacuum distillation is another method that can be used to treat the waste acid. Although the energy consumption is greatly saved compared with the normal temperature distillation, the low-boiling organic matter in the waste acid will be precipitated in the condensation pipe during direct distillation, which will cause blockage. At the same time, it seriously affects the heat transfer efficiency of the condenser, which greatly limits the application of this method
For the treatment of copper-containing waste acid, there is no report on industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 500ml of filtered waste acid and place it in a 1000ml beaker, add 0.1g of potassium permanganate and 3ml of sodium hypochlorite, stir and react for 20 minutes, the color of the waste acid becomes darker at the beginning, and then turns back to green. After the reaction, there is no floc A small amount of brown suspended matter floats on the surface of the acid liquid. The suspension was filtered off, and vacuum distillation was carried out in a 1000ml distillation flask under a vacuum of 0.08Mpa. The initial boiling point temperature is 80°C, and the end point temperature is 87°C. Dilute hydrochloric acid with a stock solution volume of 85% was obtained, the concentration of hydrochloric acid was 12.6%, and almost no floc appeared in the condensation tube. This shows that the composite oxidant of potassium permanganate and sodium hypochlorite has oxidized the low-boiling point organic matter, and the effect is better.

Embodiment 2

[0019] Take 2000L of waste acid liquid for pilot test in an enamel kettle, add 450g of potassium permanganate and 12L of sodium hypochlorite, carry out oxidation reaction for 20 minutes under stirring, and distill under reduced pressure at 0.07Mpa. 85% dilute hydrochloric acid, the concentration of hydrochloric acid is 13.5%, and there is almost no floc in the condensation tube. This shows that the oxidation process can oxidize low-boiling organic matter in industrial-scale waste acid liquid, which fully meets the requirements of industrial vacuum distillation.

Embodiment 3

[0021] Take 500ml of the above-mentioned 13% dilute hydrochloric acid and place it in a 1000ml distillation bottle, add 5% CaCl 2 Carry out extractive distillation, vacuum degree is 0.07Mpa, boiling point temperature is 92 ℃, obtains 30% hydrochloric acid 400ml. This shows that the extraction concentration distillation method of the present invention can improve the concentration of hydrochloric acid from 13% to 30%.

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PUM

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Abstract

The present invention provides one waste copper containing acid solution recovering and utilizing process in saccharin sodium production. The waste copper containing acid solution recovering and utilizing process includes filtering to eliminate suspended organic matter, oxidizing the filtrate with mixed oxidant of sodium hypochlorite and potassium hypermanganate to eliminate low boiling point organic matter, decompression distilling the solution in vacuum to obtain dilute hydrochloric acid solution, further extraction and concentrating distillation to obtain hydrochloric acid solution of 30 % concentration, burning residue after decompression distilling to eliminate organic matter and obtain high purity copper sulfate and powder of other inorganic salts. The said process can recover the useful matter from waste acid solution and avoid environmental pollution effectively.

Description

Technical field: [0001] The invention relates to a method for recycling copper-containing waste acid liquid in the production of sodium saccharin. The useful substances in the waste acid liquid are recovered through oxidation, vacuum distillation and extraction concentration distillation, and the pollution of the waste to the environment is eliminated. Background technique: [0002] During the replacement and chlorination processes in the production of sodium saccharin, copper sulfate is used as a catalyst to produce mixed acidic water containing copper salt, sodium chloride, sodium bisulfate, sulfuric acid, and hydrochloric acid. The mass fraction of copper ions in the acidic water is about 1%, hydrochloric acid is about 5%, and sulfuric acid is about 9%. The treatment of this wastewater is mostly using the iron replacement method at present. Iron is added to copper waste liquid to reduce and recover copper. However, the remaining acid liquid contains ferrous sulfate, whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/02C02F9/04
Inventor 杨庆峰张振家
Owner SHANGHAI JIAO TONG UNIV
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